US4040863A - Method of treating surface of copper and its alloys - Google Patents
Method of treating surface of copper and its alloys Download PDFInfo
- Publication number
- US4040863A US4040863A US05/735,442 US73544276A US4040863A US 4040863 A US4040863 A US 4040863A US 73544276 A US73544276 A US 73544276A US 4040863 A US4040863 A US 4040863A
- Authority
- US
- United States
- Prior art keywords
- copper
- solution
- alloys
- chlorine ion
- cyclohexanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
Definitions
- This invention relates to a method of chemical surface treatment of copper and its alloys with an acidic aqueous solution of hydrogen peroxide in which hindering action of dissolved chlorine ion in removal of the metals and oxide scales by dissolution is inhibited. More particularly, it is directed to inhibiting the hindering action of dissolved chlorine ion in the chemical surface treatment of copper and its alloys such as the pcikling, etching or chemical polishing for which an acidic aqueous solution of hydrogen peroxide is used by adding to the solution methylcyclohexanol or cyclohexanol or both of the two.
- the acidic aqueous solution of hydrogen peroxide has an excellent dissolving activity as a chemical surface-treating agent for copper and copper-alloy materials.
- chlorine ion when there is incorporated chlorine ion at 1 p.p.m. or more in the solution, the metal- or oxide scale-dissolving activity will be greatly reduced with unsatisfactory finishing of the pickling, etching or chemical polishing resulted.
- a method in which a silver compound such as silver nitrate or sulfate is added to remove the incorporated chlorine ion as precipitates of inactive silver chloride. In the method, however, it is difficult to add the silver ion in an amount equivalent to the chlorine ion. If the silver ion is added in excess, silver will be precipitated upon the surface of copper and its alloys with an disadvantage that dissolution of the metal or oxide scale is undesirably inhibited.
- the present invention which is based upon the above-mentioned finding, provides a method of inhibiting the hindrance superior to any of the known methods of inhibiting the hindering action of chlorine ion.
- the aqueous hydrogen-peroxide solution used for the chemical surface treatments of copper and its alloys contains 10-150 g./l. of hydrogen peroxide, 10-200 g./l. of sulfuric acid, and additionally, a stabilizer for hydrogen peroxide and a surface active agent.
- the solution which is a very effective surface-treating agent in the absence of chlorine ion, will be extremely deteriorated in activity of dissolving the metals and oxide scales and lose the chemical polishing activity if chlorine ion is incorporated from diluent water or others.
- This invention is concerned with a method of inhibiting the action of chlorine ion hindering removal of copper and its alloys and their oxide scales by addition of methylcyclohexanol or cyclohexanol or both of the two to an acidic aqueous solution of hydrogen peroxide, according to which method it is feasible to employ water containing chlorine ion.
- addition of methylcyclohexanol or cyclohexanol or both of the two in an amount of 0.1 g./l. or more produces the expected results though the amount less than 0.1 g./l. will produce some but unsatisfactory results.
- the effect will be increased with increase in the amount added up to a nearly constant effect at 5 g./l. There will be no problem with the addition more than 5 g./l. but it is uneconomical.
- the acid employed in the method of the invention includes mineral acids excluding hydrochloric acid such as sulfuric, nitric and phosphoric acids.
- a hydrogen peroxide-decomposition inhibitor including glycol ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether and ethylene glycol monobutyl ether, saturated aliphatic alcohols such as methyl alcohol, ethyl alcohol and butyl alcohol, carboxylic acids, amino carboxylic acids and phosphonic acids.
- glycol ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether and ethylene glycol monobutyl ether
- saturated aliphatic alcohols such as methyl alcohol, ethyl alcohol and butyl alcohol
- carboxylic acids amino carboxylic acids and phosphonic acids
- the metal-treating temperature between 20 and 50° C. is suitable. At lower temperatures, the expected results will not satisfactorily be produced, while higher temperatures is undesirable because of promotion of decomposition of the hydrogen peroxide with a shorter life of the treating solution resulted.
- a brass plate (Cu 60, Zn 40) with oxide coating was treated by dipping in an aqueous solution containing 20 g./l. of H 2 O 2 , 70 g./l. of HNO 3 , 10 ml./l. of ethylene glycol monoethyl ether, 1 g./l. of a non-ionic surface active agent and 5 ppm of Cl - at 40° C. for 1 minute. Removal of the oxide coating was not satisfactory.
- a beryllium-copper alloy plate was treated by dipping in an aqueous solution containing 50 g./l. of H 2 O 2 , 40 g./l. of H 2 SO 4 , 20 g./l. of HNO 3 , 50 ml./l. of methyl alcohol, 2 ml./l. of a non-ionic surface active agent and 5 ppm of Cl - at 25° C. for about 2 min. There was produced black stripes on the surface.
- a pure copper plate with oxide coating was dipped in an aqueous solution containing 40 g./l. of H 2 O 2 , 150 g./l. of H 2 SO 4 , 50 ml./l. of ethyl alcohol, 0.5 g./l. of a non-ionic surface active agent and a predetermined amount of chlorine ion at 40° C. for about 1 minute.
- the results are shown in Table 1.
- Comparative Example 1 To the solution of Comparative Example 1 was added cyclohexanol at 0.5 g./l. In the resulting solution at 40° C. was dipped a brass plate (Cu 60, Zn 40) with oxide coating for about 1 minute. Removal of the oxide coating was good.
- Comparative Example 2 To the solution of Comparative Example 2 was added methylcyclohexanol at 1 g./l. In the resulting solution at 25° C. was dipped a beryllium-copper alloy plate for about 2 minutes. There was produced a glazed surface.
- a pure copper plate was dipped in an aqueous solution containing 100 g./l. of H 2 O 2 , 100 g./l. of H 2 SO 4 , 20 ml./l. of ethylene glycol monomethyl ether, 1 g./l. of a non-ionic surface active agent, 50 ppm of Cl - and 5 g./l. of cyclohexanol at 45° C. for 10 sec. There was produced a glazed surface.
- a pure copper plate with oxide coating was dipped in an aqueous solution containing 40 g./l. of H 2 O 2 , 150 g./l. of H 2 SO 4 , 50 ml./l. of ethyl alcohol, 0.5 g./l. of a non-ionic surface active agent, 5-50 ppm of Cl - and 0.1 - 5 g./l. of methylcyclohexanol at 40° C. for about 1 minute. Results of the treatment are shown in Table 3.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Chemical Treatment Of Metals (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP273776A JPS5286933A (en) | 1976-01-14 | 1976-01-14 | Method of treating surface of copper and copper alloy |
JA51-2737 | 1976-01-14 |
Publications (1)
Publication Number | Publication Date |
---|---|
US4040863A true US4040863A (en) | 1977-08-09 |
Family
ID=11537636
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US05/735,442 Expired - Lifetime US4040863A (en) | 1976-01-14 | 1976-10-26 | Method of treating surface of copper and its alloys |
Country Status (13)
Country | Link |
---|---|
US (1) | US4040863A (ja) |
JP (1) | JPS5286933A (ja) |
BE (1) | BE850248A (ja) |
CA (1) | CA1075570A (ja) |
CH (1) | CH624995A5 (ja) |
DE (1) | DE2701409A1 (ja) |
ES (1) | ES455003A1 (ja) |
FR (1) | FR2338335A1 (ja) |
GB (1) | GB1547041A (ja) |
IT (1) | IT1076212B (ja) |
NL (1) | NL7700370A (ja) |
NO (1) | NO144156C (ja) |
SE (1) | SE428477B (ja) |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4158593A (en) * | 1977-11-08 | 1979-06-19 | Dart Industries Inc. | Dissolution of metals utilizing a H2 O2 -sulfuric acid solution catalyzed with selenium compounds |
US4174253A (en) * | 1977-11-08 | 1979-11-13 | Dart Industries Inc. | Dissolution of metals utilizing a H2 O2 -H2 SO4 solution catalyzed with hydroxy substituted cycloparaffins |
US4401509A (en) * | 1982-09-07 | 1983-08-30 | Fmc Corporation | Composition and process for printed circuit etching using a sulfuric acid solution containing hydrogen peroxide |
US4462861A (en) * | 1983-11-14 | 1984-07-31 | Shipley Company Inc. | Etchant with increased etch rate |
US4754803A (en) * | 1987-02-02 | 1988-07-05 | Phelps Dodge Industries, Inc. | Manufacturing copper rod by casting, hot rolling and chemically shaving and pickling |
US4826544A (en) * | 1987-12-22 | 1989-05-02 | Essex Group, Inc. | Hydrogen cleaning of hot copper rod |
US4946520A (en) * | 1987-02-02 | 1990-08-07 | Phelps Dodge Industries, Inc. | Copper rod manufactured by casting, hot rolling and chemically shaving and pickling |
US5030373A (en) * | 1989-03-08 | 1991-07-09 | Tokai Denka Kogyo Kabushiki Kaisha | Surface-treating agents for copper and copper alloy |
US5211927A (en) * | 1990-11-27 | 1993-05-18 | Tokai Denka Kogyo Kabushiki Kaisha | Method for stabilizing acidic aqueous hydrogen peroxide solution containing copper |
EP0816532A2 (en) * | 1996-06-27 | 1998-01-07 | Ykk Corporation | Method for production of slide fastener or stringers thereof |
US6803354B2 (en) | 2002-08-05 | 2004-10-12 | Henkel Kormanditgesellschaft Auf Aktien | Stabilization of hydrogen peroxide in acidic baths for cleaning metals |
US20050126918A1 (en) * | 2003-12-11 | 2005-06-16 | Industrial Technology Research Institute | Surface treatment process for enhancing a release rate of metal ions from a sacrificial electrode and a related sacrificial electrode |
US20060289034A1 (en) * | 2003-12-31 | 2006-12-28 | Small Robert J | Compositions containing free radical quenchers |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4141850A (en) * | 1977-11-08 | 1979-02-27 | Dart Industries Inc. | Dissolution of metals |
JPS5540484A (en) * | 1978-09-15 | 1980-03-21 | Sumitomo Electric Ind Ltd | Reinforcing method of optical fiber connecting part |
US4437927A (en) * | 1983-08-22 | 1984-03-20 | Dart Industries Inc. | Dissolution of metals utilizing a lactone |
US4437928A (en) * | 1983-08-22 | 1984-03-20 | Dart Industries Inc. | Dissolution of metals utilizing a glycol ether |
DE4402788A1 (de) * | 1994-01-31 | 1995-08-10 | Emil Krechen Industrievertretu | Verfahren zum Abtragen von Metallen |
JP2013199702A (ja) * | 2012-02-24 | 2013-10-03 | Mitsubishi Shindoh Co Ltd | 銅或いは銅基合金表面の酸化皮膜の除去方法 |
JP6516214B2 (ja) * | 2015-03-20 | 2019-05-22 | パナソニックIpマネジメント株式会社 | 多層膜用エッチング液とエッチング濃縮液およびエッチング方法 |
CN107690488B (zh) * | 2016-09-09 | 2019-03-01 | 松下知识产权经营株式会社 | 多层膜用蚀刻液和蚀刻浓缩液及蚀刻方法 |
TW202208686A (zh) * | 2020-06-08 | 2022-03-01 | 日商三菱瓦斯化學股份有限公司 | 用於銅或銅合金之表面處理的化學研磨液及表面處理方法 |
Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3293093A (en) * | 1963-12-30 | 1966-12-20 | Allied Chem | Dissolution of metal with acidified hydrogen peroxide and use as copper etchant in manufacture of printed circuits |
US3483050A (en) * | 1966-03-17 | 1969-12-09 | Allied Chem | Acid-peroxide dissolution of metals in the presence of titanium |
US3556883A (en) * | 1967-07-21 | 1971-01-19 | Mitsubishi Edogawa Kagaku Kk | Method for chemically polishing copper or copper alloy |
US3597290A (en) * | 1968-03-25 | 1971-08-03 | Mitsubishi Edogawa Kagaku Kk | Method for chemically dissolving metal |
US3635836A (en) * | 1969-11-10 | 1972-01-18 | Gen Mills Inc | Thickened compositions and the process of preparing same |
US3649194A (en) * | 1969-10-28 | 1972-03-14 | Fmc Corp | Stabilization of acidified hydrogen peroxide solutions |
US3864271A (en) * | 1972-12-04 | 1975-02-04 | Du Pont | Stabilized acidic hydrogen peroxide solutions |
US3869401A (en) * | 1972-12-04 | 1975-03-04 | Du Pont | Stabilized acidic hydrogen peroxide solutions |
US3905907A (en) * | 1972-12-22 | 1975-09-16 | Furukawa Electric Co Ltd | Solutions for chemical dissolution treatment of metal materials |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1420043A (fr) * | 1964-12-24 | 1965-12-03 | Allied Chem | Procédé d'utilisation du peroxyde d'hydrogène pour l'attaque chimique du cuivre, en particulier pour la fabrication de circuits imprimés |
FR1539960A (fr) * | 1967-08-11 | 1968-09-20 | Mitsubishi Edogawa Kagaku Kk | Procédé de polissage du cuivre ou des alliages de cuivre |
-
1976
- 1976-01-14 JP JP273776A patent/JPS5286933A/ja active Granted
- 1976-10-26 US US05/735,442 patent/US4040863A/en not_active Expired - Lifetime
-
1977
- 1977-01-05 CA CA269,152A patent/CA1075570A/en not_active Expired
- 1977-01-10 BE BE173972A patent/BE850248A/xx not_active IP Right Cessation
- 1977-01-10 NO NO770073A patent/NO144156C/no unknown
- 1977-01-13 FR FR7700931A patent/FR2338335A1/fr active Granted
- 1977-01-13 IT IT19280/77A patent/IT1076212B/it active
- 1977-01-13 CH CH43177A patent/CH624995A5/de not_active IP Right Cessation
- 1977-01-13 ES ES455003A patent/ES455003A1/es not_active Expired
- 1977-01-14 SE SE7700391A patent/SE428477B/xx unknown
- 1977-01-14 GB GB1577/77A patent/GB1547041A/en not_active Expired
- 1977-01-14 NL NL7700370A patent/NL7700370A/xx not_active Application Discontinuation
- 1977-01-14 DE DE19772701409 patent/DE2701409A1/de not_active Withdrawn
Patent Citations (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3293093A (en) * | 1963-12-30 | 1966-12-20 | Allied Chem | Dissolution of metal with acidified hydrogen peroxide and use as copper etchant in manufacture of printed circuits |
US3483050A (en) * | 1966-03-17 | 1969-12-09 | Allied Chem | Acid-peroxide dissolution of metals in the presence of titanium |
US3556883A (en) * | 1967-07-21 | 1971-01-19 | Mitsubishi Edogawa Kagaku Kk | Method for chemically polishing copper or copper alloy |
US3597290A (en) * | 1968-03-25 | 1971-08-03 | Mitsubishi Edogawa Kagaku Kk | Method for chemically dissolving metal |
US3649194A (en) * | 1969-10-28 | 1972-03-14 | Fmc Corp | Stabilization of acidified hydrogen peroxide solutions |
US3635836A (en) * | 1969-11-10 | 1972-01-18 | Gen Mills Inc | Thickened compositions and the process of preparing same |
US3864271A (en) * | 1972-12-04 | 1975-02-04 | Du Pont | Stabilized acidic hydrogen peroxide solutions |
US3869401A (en) * | 1972-12-04 | 1975-03-04 | Du Pont | Stabilized acidic hydrogen peroxide solutions |
US3905907A (en) * | 1972-12-22 | 1975-09-16 | Furukawa Electric Co Ltd | Solutions for chemical dissolution treatment of metal materials |
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4158593A (en) * | 1977-11-08 | 1979-06-19 | Dart Industries Inc. | Dissolution of metals utilizing a H2 O2 -sulfuric acid solution catalyzed with selenium compounds |
US4174253A (en) * | 1977-11-08 | 1979-11-13 | Dart Industries Inc. | Dissolution of metals utilizing a H2 O2 -H2 SO4 solution catalyzed with hydroxy substituted cycloparaffins |
US4401509A (en) * | 1982-09-07 | 1983-08-30 | Fmc Corporation | Composition and process for printed circuit etching using a sulfuric acid solution containing hydrogen peroxide |
US4462861A (en) * | 1983-11-14 | 1984-07-31 | Shipley Company Inc. | Etchant with increased etch rate |
US4754803A (en) * | 1987-02-02 | 1988-07-05 | Phelps Dodge Industries, Inc. | Manufacturing copper rod by casting, hot rolling and chemically shaving and pickling |
US4946520A (en) * | 1987-02-02 | 1990-08-07 | Phelps Dodge Industries, Inc. | Copper rod manufactured by casting, hot rolling and chemically shaving and pickling |
US4826544A (en) * | 1987-12-22 | 1989-05-02 | Essex Group, Inc. | Hydrogen cleaning of hot copper rod |
US5030373A (en) * | 1989-03-08 | 1991-07-09 | Tokai Denka Kogyo Kabushiki Kaisha | Surface-treating agents for copper and copper alloy |
US5211927A (en) * | 1990-11-27 | 1993-05-18 | Tokai Denka Kogyo Kabushiki Kaisha | Method for stabilizing acidic aqueous hydrogen peroxide solution containing copper |
EP0816532A2 (en) * | 1996-06-27 | 1998-01-07 | Ykk Corporation | Method for production of slide fastener or stringers thereof |
EP0816532A3 (en) * | 1996-06-27 | 1998-01-14 | Ykk Corporation | Method for production of slide fastener or stringers thereof |
US6245251B1 (en) | 1996-06-27 | 2001-06-12 | Ykk Corporation | Method for production of slide fastener or stringers thereof |
US6803354B2 (en) | 2002-08-05 | 2004-10-12 | Henkel Kormanditgesellschaft Auf Aktien | Stabilization of hydrogen peroxide in acidic baths for cleaning metals |
US20050126918A1 (en) * | 2003-12-11 | 2005-06-16 | Industrial Technology Research Institute | Surface treatment process for enhancing a release rate of metal ions from a sacrificial electrode and a related sacrificial electrode |
US7118665B2 (en) * | 2003-12-11 | 2006-10-10 | Industrial Technology Research Institute | Surface treatment process for enhancing a release rate of metal ions from a sacrificial electrode and a related sacrificial electrode |
US20060289034A1 (en) * | 2003-12-31 | 2006-12-28 | Small Robert J | Compositions containing free radical quenchers |
Also Published As
Publication number | Publication date |
---|---|
NO144156C (no) | 1981-07-01 |
IT1076212B (it) | 1985-04-27 |
JPS5323244B2 (ja) | 1978-07-13 |
GB1547041A (en) | 1979-06-06 |
SE7700391L (sv) | 1977-07-15 |
ES455003A1 (es) | 1978-04-01 |
FR2338335A1 (fr) | 1977-08-12 |
CH624995A5 (ja) | 1981-08-31 |
JPS5286933A (en) | 1977-07-20 |
BE850248A (fr) | 1977-07-11 |
NL7700370A (nl) | 1977-07-18 |
FR2338335B1 (ja) | 1980-04-18 |
CA1075570A (en) | 1980-04-15 |
SE428477B (sv) | 1983-07-04 |
NO144156B (no) | 1981-03-23 |
NO770073L (no) | 1977-07-15 |
DE2701409A1 (de) | 1977-07-28 |
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